CN101371381B - A method of fabricating fibres composed of silicon or a silicon-based material and their use in lithium rechargeable batteries - Google Patents
A method of fabricating fibres composed of silicon or a silicon-based material and their use in lithium rechargeable batteries Download PDFInfo
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- CN101371381B CN101371381B CN2007800029760A CN200780002976A CN101371381B CN 101371381 B CN101371381 B CN 101371381B CN 2007800029760 A CN2007800029760 A CN 2007800029760A CN 200780002976 A CN200780002976 A CN 200780002976A CN 101371381 B CN101371381 B CN 101371381B
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 73
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- 239000010703 silicon Substances 0.000 title claims description 72
- 229910052744 lithium Inorganic materials 0.000 title claims description 17
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 16
- 239000002210 silicon-based material Substances 0.000 title abstract description 4
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 238000005530 etching Methods 0.000 claims abstract description 12
- 239000011149 active material Substances 0.000 claims abstract description 10
- 239000000835 fiber Substances 0.000 claims description 70
- 238000000034 method Methods 0.000 claims description 54
- 239000000463 material Substances 0.000 claims description 19
- 229910001416 lithium ion Inorganic materials 0.000 claims description 15
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000003792 electrolyte Substances 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229910012851 LiCoO 2 Inorganic materials 0.000 claims description 2
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims description 2
- 229910015645 LiMn Inorganic materials 0.000 claims description 2
- 229910000577 Silicon-germanium Inorganic materials 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 229910001463 metal phosphate Inorganic materials 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 238000001020 plasma etching Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 claims 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims 2
- UULWTPBMBYVDGA-UHFFFAOYSA-N [Co](=O)=O.[Li] Chemical compound [Co](=O)=O.[Li] UULWTPBMBYVDGA-UHFFFAOYSA-N 0.000 claims 1
- 238000003486 chemical etching Methods 0.000 claims 1
- 230000008021 deposition Effects 0.000 claims 1
- 238000007790 scraping Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 239000010408 film Substances 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000002033 PVDF binder Substances 0.000 description 6
- 239000010405 anode material Substances 0.000 description 6
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000005266 casting Methods 0.000 description 3
- 229910021450 lithium metal oxide Inorganic materials 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000004087 circulation Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000011244 liquid electrolyte Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 101100317222 Borrelia hermsii vsp3 gene Proteins 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- 240000007762 Ficus drupacea Species 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- LEVVHYCKPQWKOP-UHFFFAOYSA-N [Si].[Ge] Chemical compound [Si].[Ge] LEVVHYCKPQWKOP-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000006138 lithiation reaction Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- -1 organic carbonate ester Chemical class 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
A method of fabricating fibres of silicon or silicon-based material comprises the steps of etching pillars on a substrate and detaching them. A battery anode can then be created by using the fibres as the active material in a composite anode electrode.
Description
Technical field
The present invention relates to method and the application in the active anode material of chargeable lithium cell (battery cell) thereof of the fiber that a kind of manufacturing forms by silicon or based on the material of silicon.
Background technology
Know active anode material that silicon can be used as the chargeable lithium ion electrochemical cell (for example referring to Insertion Electrode Materials for Rechargeable Lithium Batteries, M.Winter, J.O.Besenhard, M.E.Spahr and P.Novak are at Adv.Mater.1998,10, No.10).The basic composition of conventional Li-ion rechargeable cell has been shown in Fig. 1, and it comprises will be with the composition that replaces based on the anode of the silicon anode based on graphite.But this cell comprises single monomer also can comprise a plurality of monomers.
Cell generally includes suitably and outsidely to be connected in load or to recharge the copper collector that is used for anode 10 in source and be used for the aluminum current collector of negative electrode 12.Composite anode layer 14 based on graphite covers current-collector 10, and covers current-collector 12 based on the composite cathode layer 16 that contains lithium metal oxide.Based on the composite anode layer 14 of graphite with between based on the composite cathode layer 16 that contains lithium metal oxide, porous plastics dividing plate or slider 20 are being set, the liquid electrolyte dispersion of materials is in porous plastics dividing plate or slider 20, composite anode layer 14 and composite cathode layer 16.Under certain situation, porous plastics dividing plate or slider 20 can be aggregated the thing electrolyte and replace, and polymer electrolyte all occurs in these cases in composite anode layer 14 and composite cathode layer 16.
When cell charged fully, lithium was transferred to layer based on graphite, itself and graphite reaction formation compound L iC there through electrolyte from containing lithium metal oxide
6Heap(ed) capacity as the graphite of electrochemical active material in composite anode layer is 372mAh/g.Note, the term that uses " anode " and " negative electrode " refer to that battery is placed in the situation between load two ends.
It has been generally acknowledged that, when as the active anode material in the Li-ion rechargeable cell, the graphite that the Capacity Ratio of silicon is commonly used is much bigger.When Si by with the electrochemical single battery in the lithium reaction conversions be compound L i
21Si
5The time, the capacity of silicon is 4,200mAb/g.
Existingly use silicon or fail to provide the continuous rating in the requirement charge/discharge cycle therefore commercially infeasible based on the method for the active anode material of silicon in lithium ion electrochemical cells.
A kind of method adopts pulverous silicon, and it is formed the compound that has alternatively electronic additive and comprises the proper adhesive that is coated on copper collector, for example polyvinylidene fluoride in some instances.But this electrode can not provide continuous rating in charge/discharge cycle.Think that this capacitance loss is owing to embedding body silicon/extract from body silicon mechanical separation of part of relevant volumetric expansion/Si powder quality that contractions causes with lithium.This causes again powder quality gathering in electric insulation " island ".
By people such as Ohara in the another kind of method described in Journal of Power Sources 136 (2004) 303-306, silicon is formed film by evaporation to the nickel foil current-collector, and then utilizes this structure to form the anode of lithium ion battery.But, although the method can produce good capability retention, but only just like this for very thin film, so these structures can not produce the capacity of available quantity on unit are, make good capability retention eliminate and improve film thickness with the capacity that forms available quantity on unit are.
In the another kind of method described in US2004/0126659, then silicon extremely be used to form on the nickel fiber of Anode of lithium cell by evaporation.But find that it has formed the therefore obviously impact operation of the uneven distribution of silicon on the nickel fiber.
At US6, in the another kind of method described in 887,511, silicon is by the extremely coarse interior thickness film based on formation 10 μ m at the end of copper of evaporation.Embed the lithium ion process initial, silicon fiml is broken and form the silicon post.Then these posts reversibly react with lithium ion and obtain good capability retention.But this process is moved bad and formed the interior thickness film thicker film is a kind of process of costliness.Thereby the broken formed column structure of film does not have inherent this tissue of porousness and can keep long-term capability retention in addition.
Summary of the invention
Listed the present invention in claims.Because anode electrode structure adopts based on the material of silicon or the fiber of silicon, these silicon or be overcome based on the fiber of silicon and the reversible reaction problem of lithium.Particularly by fiber is set in composite construction, i.e. the mixture of polymer adhesive and electronic additive, that charge/discharge process becomes is reversible, can repeat and obtain good capability retention.In addition, the mode that fiber wherein is set also has advantage.By unordered non-woven fibre pad is provided, produce completely reversibility and charging capacity and can not produce the risk that obvious machinery separates repeatably.For example, this fiber can be deposited as felt or felty texture.For composite construction, it can have other element, and perhaps felt can have simple binder or at suitable local loose of structure.
In addition, provide a kind of method for simplifying of making fiber, comprised the etching substrate to form post and splitter, a kind of reliable and high method of yield is provided.
Description of drawings
To embodiments of the invention be described by the example reference accompanying drawing now, wherein:
Fig. 1 is the schematic diagram that the cell element is shown;
Fig. 2 is the enlarged photograph according to electrode of the present invention; And
Fig. 3 shows the first cyclical voltage curve of silica fibre/PVDF/Super P combination electrode.
Embodiment
In a word, the present invention can form silicon or based on fiber or the filament of the material of silicon, and these fibers are used to form the felted electrode structure and have the composite anode structure of polymer adhesive, electronic additive (if necessary) and metal forming current-collector.Particularly, think that the silicon cell structure that consists of compound has overcome charging/discharging capacity loss problem.
For example by random or unordered or really arrange in an orderly manner, and be placed in compound fiber or felt or felty texture, namely intersect to provide many long fine fibres in a plurality of crosspoints, can alleviate charging/discharging capacity loss problem.
Usually, the length diameter ratio of fiber is approximately 100: 1, therefore anode layer for example in composite anode layer every fiber will contact other fiber repeatedly along its length, forms a kind of possible structure that wherein can ignore the machinery separation that is produced by the contact of fracture silicon.And, although can cause volumetric expansion and volume contraction, lithium is embedded fiber and can not cause fiber destruction from the fiber removal lithium, therefore kept the electronic conductivity of fibrous inside.
Can be by post be separated the manufacturing fiber with substrate.In addition, can provide the mode of making post by simple repeatably chemical technology.
A kind of mode that can form post is dry method erosion, the deep reactive ion etch described in U. S. application 10/049736 for example, and this application and the application own together, and are incorporated herein by reference.Thereby knowing this process, those skilled in the art here do not need to describe in detail.But simply, etching and the silicon base of rinsing coated native oxide are to form water-wetted surface.Cesium chloride (CsCl) by evaporation from the teeth outwards, and under drying condition with the substrate feed of coating to steam air pressure constant chamber.The CsCl film develops to the island array of hemisphere, and its size characteristic depends on original depth, steam air pressure and developing time.Island array provides a kind of effective mask, is for example carrying out by reactive ion etching the post array that etching has formed corresponding hemisphere island thereafter.CsCl resist layer height is water-soluble and easily be rinsed.
Alternatively, can be by wet etching/employings chemical electric switching method (chemical galvanic exchangemethod) formation post described in our the application GB0601318.9 of common pending trial for example, this application has common assignee, title is " Method of etching asilicon-based material ", and is incorporated herein by reference.At Peng K-Q, Yan, Y-J Gao, S-P, Zhu J., Adv.Materials, 14 (2004), 1164-1167 (" Peng "); The people such as K.Peng, Angew.Chem.Int.Ed., 442737-2742; With people such as K.Peng, Adv.Funct.Mater. discloses also spendable correlation technique in 16 (2006), 387-394.
In a preferred embodiment, for example length is that 100 microns, diameter are that the cylindricality of 0.2 micron is formed on silicon base and from silicon base and forms.More generally, length is in the post that 20 to 300 micrometer ranges, diameter or maximum transverse size be in 0.08 to 0.5 micrometer range and can be used for providing fiber.According to this technique, silicon base can be n-or p-type, and according to chemical method, it can be etched on (100) or (110) of any exposure crystal face.Because etching is carried out along crystal face, so formed fiber is monocrystal.Due to this architectural feature, it is about 100: 1 that this fiber will form length diameter ratio easily, and in being in composite anode layer the time, allows every fiber along its other fiber of length multiple-contact.Also can carry out etch process on very lagre scale integrated circuit (VLSIC) (VLSI) electron level wafer or on its sample that abandons (single-crystal wafer).As more cheap selection, also can adopt as being used for the photovoltaic grade polycrystalline material of solar panel.
For post being separated to obtain fiber, the substrate that is attached with post is placed in beaker or any suitable container, by inert fluid for example ethanol cover and be subject to ultrasonic agitation.Discovery can see that within a few minutes liquid becomes muddy, and can see at this stage post by electron microscope examination and being removed from its silicon base.
To recognize, the optional method that is used for " collections " post comprises that the substrate surface of swiping is to be isolated or with its Chemical Decomposition.The described substrate of etching in HF solution when a kind of chemical method of the n-of being suitable for type silicon materials is included in the back side illuminaton that occurs silicon wafer.
It can be used as the active material in the composite anode of lithium ion electrochemical cells in case the silicon post is separated.Be to make composite anode, filter collected silicon from solution, it can be mixed with polyvinylidene fluoride, and with casting solvent n-methyl pyrrolidone formation slurries for example.Then these slurries can for example utilize scraper physically or apply or be applied to metallic plate or metal forming or other conductive substrates with any other suitable method, the coated film that needs thickness with generation, then utilize the suitable drying system of the raising temperature that can adopt 50 ℃ to 140 ℃, casting solvent is evaporated from this film, to stay the composite membrane that does not have or substantially there is no casting solvent.The pad that produces or composite membrane have porous and/or felty texture, and wherein the quality of silica fibre accounts for 70% and 95% usually.The pore volume percentage of composite membrane is 10-30%, is preferably approximately 20%.
Fig. 2 shows the SEM of the combined electrode structure that obtains by top method.Alternatively, felt or felty texture can form sheet material (not necessarily on current-collector) and also be used as the current-collector of itself.
Thereafter can be for example according to general structure illustrated in fig. 1 but with silicon or based on the active anode material of silicon but not the graphite active anode material is made the lithium ion single battery with suitable method.The composite anode layer that is for example covered based on silica fibre by porous barrier 18, the electrolyte that adds final structure to is full of whole enterable pore volumes.Add electrolyte after electrode is placed in suitable shell, described interpolation can comprise the vacuum filling anode, is filled liquid electrolyte to guarantee pore volume.
Please refer to following example:
The silica fibre of weighing 0.0140g is put into 2cm
2The Eppendorf centrifuge tube in, and the Super P conductive carbon of adding 0.0167g.Then 1-METHYLPYRROLIDONE (NMP) is moved in pipe until disperse all materials (0.92g).In advance, the PVDF of 7.8wt% is dissolved in NMP.This solution that will contain 0.0074g PVDF is added into pipe.The following Si of blending constituent: PVDF: Super P=85.3: 4.5: 10.1wt%.
This pipe is placed in and reaches one hour in ultrasonic tank so that this mixture is even, and then stirs one hour.Then adopting scraper gap is that the scraper of 0.8mm is applied to these slurries on the Copper Foil of 14 μ m.Then under 100 ℃ to dry one hour of this coating with the evaporation nmp solvent.After super-dry, the thickness of coating is 30-40 μ m.Fig. 2 shows the similar mixture that there is no Super P carbon and the SEM of coating.
Rolling coating gently, then electrode disk be cut for diameter be 12mm.In the glove box of argon filling is assembled to electrochemical cell with it.Counterelectrode and reference electrode are all the lithium metal.Electrolyte is the LiPF in the organic carbonate ester admixture
6This battery of test on VMP3 equipment.Through after halfhour immersion, this battery is maintained at-and 0.1mA reaches one hour, and then acquisitions-0.2mA is until the lithiation capacity of needs.Then+0.2mA takes off lithiumation to electrode, until 1.0V vs.Li/Li
+Voltage.Fig. 3 shows the cell voltage in this first circulation.
Here the special advantage of institute's describing method be if necessary can to make, the anode based on silicon of rolling sheet, then the samely cut subsequently or punching press with the anode based on graphite of current lithium ion single battery, this means that method as described herein can improve with existing manufacturing capacity.
Here describe another advantage that arranges and be that structural strength is in fact along with each charging operations improves.This is because because the crystal structure that breaks on the fiber node that forms impalpable structure causes fiber " fusion " mutually.This has reduced again the risk of capacitance loss in a plurality of circulations, in case this be that fibre machinery separates because fiber connects in the above described manner may be lower.
Certainly, can adopt any suitable method to realize said method and device with understanding.For example, the post lock out operation can comprise shake, swipe, chemistry or other operation any, as long as remove post to form fiber from substrate.When suitable, the reference based on the material of silicon is comprised silicon.This fiber can have any suitable size, and for example can be for the silicon of pure silicon or doping or other based on the material of silicon for example silicon-germanium mixture or any other suitable mixture.The substrate that forms post can be n-or p-type, from 100 to 0.001 ohm of cm, and perhaps it can be suitable silicon alloy, for example Si
xGe
1-xFiber can be used for any suitable purpose and for example makes the electrode that generally includes negative electrode.This cathode material can be any suitable material, is generally metal oxide or phosphate material based on lithium, for example LiCoO
2, LiMn
xNi
xCo
1-2xO
2Perhaps LiFePO
4The feature of different embodiment can mutually replace or be set up in parallel and carry out the method step with any suitable order.
Claims (37)
1. a manufacturing is used for the method for the electrode of lithium ion battery, described electrode comprise silicon or based on the fiber of the material of silicon as active material, described method comprise the steps: the etching silicon substrate or based on the substrate of silicon to form post; Described post is separated to form described silicon or based on the fiber of the material of silicon from described substrate; And described fiber is set to the active material of the electrode of lithium ion battery.
2. according to claim 1 method, the lateral dimension of wherein said fiber is in the scope of 0.08 to 0.5 micron, and its length is in the scope of 20 to 300 microns.
3. according to claim 2 method, the lateral dimension of wherein said fiber is 0.2 micron, and its length is 100 microns.
4. according to claim 1 method, the aspect ratio of wherein said fiber is 100:1.
5. the method for any one according to claim 1-4, wherein said fiber has circular cross section.
6. the method for any one according to claim 1-4, wherein said fiber has non-circular cross section.
7. according to claim 1 and 2 method, wherein form described post by reactive ion etching.
8. according to claim 1 and 2 method, wherein form described post by the chemical reaction etching.
9. according to claim 8 method, wherein form described post by the electrochemical exchange etching.
10. according to claim 1 and 2 method wherein separates described post by one or more of scraping, stirring or chemical etching.
11. method according to claim 1 and 2, wherein said silicon or comprise a kind of in undoped silicon, doped silicon or SiGe mixture based on the material of silicon.
12. method according to claim 1 and 2, wherein said fiber are monocrystalline silicon.
13. a method that is formed for the complexes membrane electrode of lithium ion battery, described method comprises:
To have 0.08 to 0.5 micron lateral dimension silicon or mix to form compound based on the fiber of silicon with adhesive and/or electronic additive;
Deposition comprises the slurries of described compound;
Form silicon or based on the layer of the fiber of silicon as described complexes membrane electrode, wherein said fiber forms felt, wherein said felt comprises the layer of random, unordered or orderly fiber, described fiber layer be set to provide a plurality of crosspoints between fiber; And
Form the amorphous silicon part on fiber intersection points.
14. method according to claim 13, wherein said fiber are mono-crystlling fibre.
15. according to claim 13 or 14 method, wherein form described silicon or comprise based on the step of the layer of the fiber of silicon and form the felted layer.
16. according to claim 13 or 14 method comprises described slurries are deposited on current-collector.
17. according to claim 13 or 14 method, wherein by the etching silicon substrate or based on the substrate of silicon to form post and described post separated to form described silicon or based on the fiber of silicon from described substrate.
18. according to claim 13 or 14 method, wherein said electrode are anode.
19. according to claim 13 or 14 method, the pore volume percentage of wherein said complexes membrane electrode is 10-30%.
20. a battery, the electrode that it comprises the method formation that utilizes any one in claim 13 to 19 also comprises negative electrode and electrolyte.
21. battery according to claim 20 also is included between described negative electrode and described electrode and adds slider.
22. according to claim 20 or 21 battery also is included in described battery shell is provided on every side.
23. an electrode that is used for lithium ion battery, described electrode comprise by the etching silicon substrate or based on the substrate of silicon to form post, described post separated to form silicon or based on a kind of silicon of making of the fiber of the material of silicon and the active material that described fiber is set to described electrode or based on the fiber of silicon from described substrate.
24. electrode according to claim 23, it uses copper to be current-collector.
25. electrode according to claim 23, wherein said electrode are anode.
26. an electrochemical cell comprises electrode as described in any one in claim 23 to 25.
27. electrochemical cell according to claim 26, it also comprises negative electrode, and described negative electrode comprises that the lithium-containing compound that can discharge and reuptake lithium ion is as its active material.
28. electrochemical cell according to claim 27, wherein said negative electrode comprise metal oxide or phosphate based on lithium as its active material.
29. electrochemical cell according to claim 28, wherein said active material are LiCoO
2Perhaps LiMn
xNi
xCo
1-2xO
2Perhaps LiFePO
4
30. compound lithium rechargeable battery anode, the layer based on the electrode fiber of silicon as the active material of electrode that comprises adhesive and/or electronic additive and have the lateral dimension of 0.08 to 0.5 micron, wherein said fiber forms felt, wherein said felt comprises the layer of random, unordered or orderly electrode fiber, the layer of described electrode fiber is set to provide a plurality of crosspoints between the electrode fiber, comprises the amorphous silicon part that is positioned on described fiber intersection points.
31. anode according to claim 30, wherein said electrode fiber is monocrystalline silicon.
32. anode according to claim 30, wherein said electrode fiber comprises N-shaped or p-type silicon.
33. anode according to claim 30, the length of wherein said electrode fiber are in the scope of 20 to 300 microns.
34. a battery comprises negative electrode and anode according to claim 30.
35. battery according to claim 34, wherein said negative electrode comprises the material based on lithium.
36. battery according to claim 34, wherein said negative electrode comprises the cobalt dioxide lithium.
37. battery powered equipment by any one according to claim 34 to 36.
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PCT/GB2007/000211 WO2007083155A1 (en) | 2006-01-23 | 2007-01-23 | A method of fabricating fibres composed of silicon or a silicon-based material and their use in lithium rechargeable batteries |
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